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A polyhedral oligomeric silsesquioxane containing hydroxyl metal tin and its preparation and application

A polysilsesquioxane, polyhedral technology, applied in the field of polyhedral oligomeric silsesquioxane, can solve the problem of no research on polymerization catalysts and the like

Active Publication Date: 2021-02-19
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, polyhedral oligomeric oligosilsesquioxanes of metallic tin containing hydroxyl groups on POSS have not been reported publicly, let alone their use as polymerization catalysts.

Method used

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  • A polyhedral oligomeric silsesquioxane containing hydroxyl metal tin and its preparation and application
  • A polyhedral oligomeric silsesquioxane containing hydroxyl metal tin and its preparation and application
  • A polyhedral oligomeric silsesquioxane containing hydroxyl metal tin and its preparation and application

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preparation example Construction

[0039] Another aspect of the present invention provides a method for preparing polyhedral oligosilsesquioxane containing hydroxyl metal tin, preferably the method for preparing the polyhedral oligomeric silsesquioxane containing hydroxyl metal tin described in the first aspect of the present invention , the method includes the following steps:

[0040] Step 1, mixing hydroxyl-containing polyhedral oligomeric silsesquioxane, an organotin compound and a solvent;

[0041] According to the present invention, in step 1, the hydroxyl-containing polyhedral oligomeric silsesquioxane is preferably the hydroxyl-containing polyhedral oligomeric silsesquioxane described in the first aspect of the present invention.

[0042] According to the present invention, in step 1, the organotin compound is preferably the organotin compound described in the first aspect of the present invention.

[0043] In the present invention, the reaction system needs to be carried out in an anhydrous environmen...

Embodiment approach

[0070] According to a preferred embodiment of the present invention, the polyhedral oligomeric silsesquioxane containing hydroxyl metal tin can be prepared by any of the following processes:

[0071]

[0072] In formula (9), R is selected from alkyl, phenyl or substituted phenyl, wherein, alkyl is selected from C 1 -C 16 Alkyl group, preferably C 1 -C 8 The alkyl group, more preferably one or more of methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl and tert-butyl, for example, R is selected from methyl, n-butyl or phenyl.

[0073]

[0074] In formula (10), R is selected from alkyl, phenyl or substituted phenyl, wherein, alkyl is selected from C 1 -C 16 Alkyl group, preferably C 1 -C 8 The alkyl group, more preferably one or more of methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl and tert-butyl, for example, R is selected from methyl, n-butyl or phenyl.

[0075]

[0076] In formula (11), R is selected from alkyl, phenyl or substituted phenyl, wherei...

Embodiment 1

[0106] 2.00g (1.87mmol) Tetrasilanolpheny POSS is joined in the 50ml reaction flask, then the reaction flask is continuously pumped and vacuumed three times, feeds nitrogen, makes the whole reaction system under the nitrogen environment, dissolves 1.22g (3.74mmol) of toluene solvent ) Bu 3 Inject SnCl into the reaction bottle, then inject 20ml of toluene solvent, and stir;

[0107] Inject 0.56ml (3.74mmol) of triethylamine into the reaction flask, and stir the reaction at 45°C for 6h to obtain the reaction product;

[0108] The reaction product was centrifuged, rotary evaporated, recrystallized in an ethanol solution of dichloromethane, and then vacuum-dried at 45°C to obtain the product, which was designated as Bu-Sn-POSS (Qt), and the yield was 85%. .

[0109] (1) Carry out infrared test to raw material Tetrasilanolpheny POSS and gained product, the infrared spectrogram that obtains is as follows figure 1 shown.

[0110] From figure 1 It can be seen that, compared with ...

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Abstract

The invention discloses polyhedral oligomeric silsesquioxane containing hydroxyl metallic tin, a preparation method and applications thereof, wherein the polyhedral oligomeric silsesquioxane containing hydroxyl metallic tin is obtained by carrying out a reaction on hydroxyl-containing polyhedral oligomeric silsesquioxane and an organic tin compound. The preparation method specifically comprises the following steps: 1, mixing hydroxyl-containing polyhedral oligomeric silsesquioxane, an organic tin compound and a solvent; 2, adding a catalyst, and carrying out a reaction to obtain a reaction product; and 3, carrying out post-treatment on the reaction product obtained in the step 2. According to the invention, by using the polyhedral oligomeric silsesquioxane containing hydroxyl metallic tinas a coordination ring-opening polymerization catalyst to catalyze and cure a cyanate ester resin and a benzoxazine resin, the curing temperature of the cyanate ester resin and the benzoxazine resin can be remarkably reduced.

Description

technical field [0001] The invention relates to the field of polyhedral oligomeric silsesquioxanes, in particular to the field of oligomeric silsesquioxanes, in particular to a double-tower polyhedral oligomeric silsesquioxane containing hydroxyl metal tin and its preparation and application. Background technique [0002] Polyhedral oligomeric silsesquioxane (Polyhedral oligomeric silsesquioxane, referred to as POSS, or T8) is a new type of nanostructure material that has emerged in recent years, and its general formula is (RSiO 1.5 )n, R can be a hydrogen atom, an alkyl group, an alkenyl group, an aryl group, etc. The chemical composition of POSS is between silica and silicate, and it is an intermediate of an intramolecular organic / inorganic hybrid structure. It has the characteristics of high melting point, low density, good dielectric properties and good thermal stability. [0003] Metal-based oligomeric silsesquioxane (POMSS) is the use of metal compounds and functional...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L79/04C08L61/34C08L83/08C08G77/398
CPCC08G77/398C08L61/34C08L79/04C08L83/08
Inventor 徐日炜包涵付琪轩余鼎声
Owner BEIJING UNIV OF CHEM TECH